基于高速喷淋法的粗四氯化锗萃取提纯工艺的研究

Study on Extraction and Purification Process of Crude Germanium Tetrachloride based on High Speed Spray Method

本研究开发了粗四氯化锗的高速喷淋萃取提纯工艺,并设计了专用的萃取试验装置,考察了萃取剂酸度、萃取相比和萃取温度对萃取效果的影响。结果表明:在萃取剂酸度为12 N,四氯化锗和萃取剂的体积比为1∶2.5,萃取夹层循环液控温5℃,萃取喷淋萃取时间为10 min,萃后静置时间为4 h的条件下,除砷率高达99.4%,锗损失率仅为0.17%;且采用萃取工艺生产出的高纯二氧化锗的品质显著高于同批次粗四氯化锗采用复蒸工艺生产的产品。

In this study,a high-speed spray extraction and purification process for crude germanium tetrachloride was developed,and a special extraction device was designed.The effects of extractant acidity,extraction ratio and extraction temperature on the extraction efficiency were investigated.The results show that the arsenic removal rate is 99.4%and germanium loss rate is only 0.17%under the conditions of extractant acidity of 12 n,volume ratio of germanium tetrachloride to extractant of 1∶2.5,temperature control of extraction interlayer circulating liquid of 5℃,extraction spray extraction time of 10 min and standing time of 4 h after extraction;And the quality of high-purity germanium dioxide produced by extraction process is significantly higher than that of crude germanium tetrachloride produced by re steaming process in the same batch.